CN109477255A - Method of the preparation for the fiber of regenerative leather substrate - Google Patents
Method of the preparation for the fiber of regenerative leather substrate Download PDFInfo
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- CN109477255A CN109477255A CN201780028381.6A CN201780028381A CN109477255A CN 109477255 A CN109477255 A CN 109477255A CN 201780028381 A CN201780028381 A CN 201780028381A CN 109477255 A CN109477255 A CN 109477255A
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-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01C—CHEMICAL OR BIOLOGICAL TREATMENT OF NATURAL FILAMENTARY OR FIBROUS MATERIAL TO OBTAIN FILAMENTS OR FIBRES FOR SPINNING; CARBONISING RAGS TO RECOVER ANIMAL FIBRES
- D01C3/00—Treatment of animal material, e.g. chemical scouring of wool
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
- C08L89/04—Products derived from waste materials, e.g. horn, hoof or hair
- C08L89/06—Products derived from waste materials, e.g. horn, hoof or hair derived from leather or skin, e.g. gelatin
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14B—MECHANICAL TREATMENT OR PROCESSING OF SKINS, HIDES OR LEATHER IN GENERAL; PELT-SHEARING MACHINES; INTESTINE-SPLITTING MACHINES
- C14B99/00—Subject matter not provided for in other groups of this subclass
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
- D02G3/10—Yarns or threads formed from collagenous materials, e.g. catgut
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Textile Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Wood Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Animal Husbandry (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Zoology (AREA)
- Sustainable Development (AREA)
- Dermatology (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
It discloses a kind of by the waste leather material method that is converted to leather fiber after industry or after consumption.This method includes acquisition with material is reduced in size to size of the length and width between about 0.5 and about 3 inch, and add surfactant by waste leather material, removal surface smoothness after the industry of surface smoothness or after consumption.After surfactant is added, the size of waste leather material is contracted to 3mm again and forms leather fiber between 9mm, and moisturizer and/or lubricant are added in the fibre, optionally after being initially opened steam.FTIR or other analytical chemistry, which can be used for before removal surface treatment identifying, to be surface-treated, this allows to select most suitable processing to remove surface treatment.
Description
Technical field
The present invention relates generally to field of compound material, including leather and adhesive, more specifically, it is preferred that emphasis is production is used
In the method for the fiber of production regenerative leather substrate.
Background technique
The various consumer goods are all made of leather and are made, including leather seat, leather wear and leather sporting goods.It was manufacturing
Cheng Zhong generates a certain amount of postindustrial waste material as leather is cut into shape.When leather and fur products is dropped, one can be also generated
Quantitative post-consumer waste.
Many trials have been carried out in history to make great efforts to simulate corium quality using waste leather in the exploitation of product.
The common application of this method is bonding leather, is the plastics being substantially made of vinyl or polyurethane, and in its backing
Contain about 17% leather fiber in material.In this material, waste leather fiber is placed in below product surface, and apply cause
Close PVC coating.Then product is struck out into hide-like appearance.It is real due to failing to establish between new material and leather
Connection, most of in these effort produce plate or paper-like material.
The primary raw material of these products is leather tanning waste material, without surface covering.It is worth noting that, being applied with surface
The Leather Waste of layer, weight are more than every year without those of billions of pounds of coating, it will usually be passed through in world's refuse landfill
Go through its end-of-life.3,000,000,000 pounds of leather garbage loading embeading is had more than every year.
It provides and is advantageous using the composition of leather waste and method after postindustrial and/or consumption, and can be used for replacing
For the leather in various products.The present invention provides such composition and methods.
Summary of the invention
Disclose the method prepared for producing the leather fiber of regenerative leather product.It also discloses and uses leather fiber system
Standby product.
This method is usually directed to after a certain amount of industry of acquisition or waste leather material after consumption, tends to surface light
Cleanliness.It ideally removes or substantially removes the surface smoothness, because once producing fiber, it is often interfered further
Procedure of processing.Therefore, the next step of this method includes processing waste leather material to remove all or substantially all surfaces
Finish.After removing finish, waste leather material is reduced to the ruler between about 0.50 inch to 3 inches of length and width
It is very little, usually square or rectangle.
Once leather substance size reduces, surfactant is just added.Surfactant can be nonionic, anion,
Cation or zwitterionic surfactant.
Once adding surfactant, the size of waste leather material reduces again, so that at least about the 92% of total fiber
Length is between 3mm and 9mm, and for the total fiber length less than 5% less than 3 millimeters, the total fiber less than 3% is more than 9 millimeters, thus
Form leather fiber.
Keep fiber humidity/lubricity be important, therefore in next step be related to leather fiber add moisturizer and/or
Lubricant.In one embodiment, before moisturizer and/or lubricant is added, fiber is opened using steam.With steam
Before processing, the water content of fiber is about usually 10 to about 30 after with steam treatment in the range of about 6 to about 8 weight %
Weight %.
Waste leather material includes but is not limited to vegetable leather, chrome leather, bark etc. after industry or after consumption.Usually exist
Synthetic polymer coating, to assign leather color or texture.Animal for its leather includes ox, goat, lamb, crocodile and short
Kiss crocodile, and after postindustrial and/or consumption waste leather often from footwear, automobile, clothes, personal leatherware, saddle manufacture or family
Tool business.
Once obtain leather source, such as industry to be regenerated after or consumption after waste leather material, this method can be further
Including obtaining the data about the polymer coating type being applied on leather, in order to its removal.Can also obtain about into
The waste leather entered receptible can handle in process of production or the data of arrangement type, and about leather color and tint
Data.
Determine that a kind of method of polymer coating type on leather is related to FTIR (Fourier transform infrared) spectrum.FTIR can
To be carried out by the way that polymer dissolution in a solvent, is then removed solvent with generating polymer.If polymer is too opaque,
It can be ground into powder, mixed with potassium bromide, thin disk is formed, for generating FTIR scanning.Execute another method of FTIR
It is using reflection FTIR, wherein IR only passes through several microns into surface to be measured.Another method is using not absorbing IR spectrum
Then the grinding agent of light in required part executes FTIR screen to scrape polymer surfaces on lapped face.
If desired, spectrum can be stored in Computer Database.It is desirable that spectrum is carried out for other library of spectra
Screening, and the type of polymer can be identified by computer matching.Although possibly can not identify a quasi polymer really
The person of being cut into, but usually every kind of polymer type will provide the FTIR spectrum with certain critical peaks, allow to identify on leather
Polymer coating type.
In this way it is possible to the data for the waste leather that every bundle relevant to the types of coatings on leather enters are obtained, and
And the information can store in the database.
Data relevant to target product requirement can also be obtained.Target data include applied to leather types of coatings with
And the chemical classes for handling leather before coating.
Certainly, the type of solvent and other conditions for removing polymer coating will change according to the property of coating.Class
As, go the processing type of leather after removing coating that will be changed according to the final use of leather.For these reasons, there is a kind of side
Method can quickly determine the optimal parameter group for removing removing coating, and be chemically treated after removing removing coating to leather.
In order to realize these targets in an efficient way, which is related to using the data with pre-stored data
Library has about the information of type of solvent and for removing the other conditions for giving polymer coating, Yi Jiguan from leather
In the pre-stored data for how handling leather fiber, once polymer is removed, so that it may performance needed for obtaining one group.Pre-defined algorithm
Or set of algorithms is for generating " updating treatment formulations ".It is discarded that the formula specifies the entrance for handling selection with further leather regeneration
The relevant bale packing information of fabric packet, and a series of leather regeneration procedural information related with processes, and it is selected for handling
A series of respective process parameter of each of the processes for the charging waste leather material packet selected is to obtain specific to target product
It is required that recycled fibrous material.
If one group of coating removal condition can be applied to a variety of different waste leathers, it can also be improved effect
Rate, therefore store information in the database and can be used for identifying those bale packing with Similar coatings, these bale packings can be with
Group is merged into row and is jointly processed by.In an embodiment of this method, by the bundle with Similar coatings before removing coating
Packet mixing.
If one group of chemical treatments can be applied in a collection of leather for therefrom having removed coating, further increase
Efficiency.Once having determined that multiple bale packings, to remove polymer coating, and have determined one group of processing to one group of condition responsive
Chemicals meets one group of performance standard of given regenerative leather product, then bale packing group merging treatment can be removed to painting
Then layer is handled to provide required performance.
Therefore, according to about the information stored in the bale packing database of " revive treatment formulations ", once selected it is big wrap into
The discarded fabric entered carries out further regeneration treatment, and selected bale packing can be subjected to being handled by the update of update treatment formulations
The specified processing step of information.In this way it is possible to obtain the recycled fibrous material specific to target product requirement.
This can be placed them into suitable reactor or blending tank, and handle for example, by opening leather substance packet
Specific leather waste is realized with removing their polymer coating.In one embodiment, resulting " clean " useless
Leather substance can mix in intimate blending step with original leather, with the leather sheet of offer " close mixing ".This process
The homogeneous mixture of all leather substances is produced, the initial stage due to leather waste in the process has unique origin,
Therefore this may be relatively important.
" cleaning " waste leather material itself is mixed with the close of original leather substance, can be carried out by cutting hides part
It is gradually reduced the process of size.
Then a series of chemistry and/or enzymatic treatment can be carried out to leather substance, may include for example making leather substance
The component of rehydration.It is, for example, possible to use natural oils, such as fat liquor, carry out rehydrated.Formic acid can be used for reducing to be dyed again
The pH value of process, and help that dyestuff chemistry product are chemically anchored on leather at the end of dye-works's process.Chrome syntans and
Chromium sulfate can use during chromium again, to improve the pliability of final leather.Resin and polymer can be used for assigning leather rich
Full scale and close texture.Dyestuff is used for colored leather, and dyeing assistant is used to help evenly dispersed dyestuff.
It may then pass through special size reducing apparatus processing fiber.This can provide the original more coordinated for Downstream processing
Material.In one embodiment, fibre length is required in 3mm between 9mm depending on downstream application.Total fiber less than 5%
It should be less than 3 millimeters long, the fiber less than 3% should be longer than 9 millimeters, and good fiber quality length is high quality non-woven fabrics leather replacement product
Required, having a size of 6 millimeters to 7 millimeters.For example, if final fiber applications are the spinning of leather yarn, best fiber
Length will be between 4mm and 6mm.
Obtained " muddy " and fibrous material can carry out further fiber adjusting, for example, using listed above
One or more chemicals, to obtain and solidify the refined fiber with required physics and chemical property.These properties can be down to
It is determined at least partially through chemicals used in selection regulating step.
Then the refined fiber of all length can be extracted for being finally packaged.
Further processing step can be carried out to convert other products, such as regenerative leather material for refined fiber,
Including complex leather material.
The present invention is better understood with reference to described in detail below.
Brief description
Fig. 1 is the overlapping diagram of the FTIR spectrum of PVC sample with the storage reference spectra of PVC.
Fig. 2 be considered the best fit of the FTIR spectrum of the sample of PVC and the PVC reference spectra of storage compared with figure
Show.Show other possible cooperations, including vinylidene chloride/vinyl chloride copolymer, carboxylation PCV, various vinyl chloride/acetic acid second
Enester/ethylene alcohol mixture, various chloride vinylacetate copolymers and inclined dichloro with different amounts of vinyl acetate
Ethylene/propene lonitrile copolymer.
Detailed description of the invention
Disclose the method prepared for producing the leather fiber of regenerative leather product.It also discloses and uses leather fiber system
At product.This regeneration techniques are intended to manufacture the leather system of high quality using all types of leather wastes, design
Feature equals or exceeds the design feature of original leather, because the engineering design of substrate is suitble to apply downstream.
In brief, this method includes the type determined for the polymer of waste after coating industry or after business, and
Optionally determine other processing for being applied to waste.By understanding the type of polymer and other processing, one can be applied
The specific treatment conditions of group remove processing, significant to be free of or the significant amount for reducing these processing so that leather composition is free of.
This makes user substantially and can be started with leather fresh, and leather is converted into required product.
However, before this, it is necessary to develop a series of conditions to remove various processing.Leather waste after postindustrial and consumption
Mainly from shoe industry, upholstery, car industry, the blue wood shavings including other kinds of transport and from process hides business.It is logical
Often but not such was the case with, and shoes waste leather is coated with polyurethane (PU) or polyvinyl chloride (PVC).Upholstery leather waste material is usually tanning
Or suede, and it is coated with PU.Automotive leather product is also tanning or suede, and is coated with PU.Blue plane from tanning operations
Spending usually has chromium oxide.
In brief, this method is related to separating scrap leather packet, and analyzes the processing type for being applied to leather.In order to from inhomogeneity
The leather fiber that high quality is created in the input of type, analyzes every batch of product, the type of analyzing polymers coating and it is optional its
His correlation process method is simultaneously recorded extremely important in database.As used herein, database is referred to as " regenerative leather number
According to library system " or " RLDS ".The strategic quality stored information in database for whole process is most important, because it is deposited
Store up and utilize the information in relation to the material to be recycled.The information of storage generally includes in the source data of the material of such as origin etc
One or more, process for tanning, complete chemicals, and/or the surface used in the cutting and sewing process of final products
Processing.These complicated quality control methods can carry out qualitative and quantization to the raw material that downstream is revived.Once raw material into
Enter RLDS, so that it may while homologous or rationally homologous material is carried out in batches and handled, to maximally utilise available
Reactor.
Once removing processed material from leather waste, resulting material can be carried out " fibrosis ", and wherein leather is cut
Or it is cut into relatively small fiber.
Other details presented below about process described herein.
I. on Leather Waste material polymer coating measurement
The surface characteristics of waste leather raw material, including but not limited to FTIR can be analyzed by one or more tests
It (Fourier Transform Infrared Spectroscopy) or is tested specific to the standard ASTM of industrial standard.
Once it is determined that surface characteristics, so that it may select one group of extraction conditions appropriate and for removing from rawhide waste material
Surfacing.Leather fiber can be restored to their nature without any apparent pollution by this.
Identify the analytical technology of polymer
FTIR (Fourier Transform Infrared Spectroscopy) is a kind of for screening and effective analysis tool of analyzing polymers sample.
FTIR test can be provided and qualitatively and quantitatively be analyzed for polymer and plastic material, such as the polymerization species for handling leather
Type.Representative ASTM scheme includes ASTM E168 and ASTM E1252.
Typical infrared scan is generated in the mid infrared region of spectrum.Mid infrared region is 400 to 4000 wave numbers,
Equal to the wavelength of 2.5 to 25 microns (10-3mm).
FTIR identifies the chemical bond in molecule by generating infrared absorption spectrum.The infrared light of material at different frequencies
It absorbs and generates unique " spectral fingerprint ", the frequency and these intensity absorbed of infrared light are absorbed based on material.Obtained spectrum
Scanning (absorbance or transmissivity) is generally specific to general material classification.For example, the spectral scan of polyurethane and the spectrum of polyester
Scanning is different, but the scanning of all polyester all has unique similitude, such as the carbonyl peak (C=O) and C-O singly-bound peak.
By by the peak match of infrared peak (the transmissivity or absorbance) infrared scan similar with known materials of material come
Complete unknown FTIR polymer identification.It is better to match, and correctly identifies that the certainty of unknown polymer is higher.
FTIR spectrum analysis can easily identify polymer classes, as nylon, polyester, polypropylene, polycarbonate, acetal or
Polyethylene.However, individually FTIR spectrum scanning should not be expected that the type of identification nylon or polyester, by polypropylene or acetal
It is identified as homopolymer or copolymer, or determines that polyethylene is high density or low density material.
Spectrum is not usually to obtain with leather sheet, because light may not pass through leather, if it is, leather
In peak all may interfere with the peak of polymer under any circumstance.However, light would generally pass through the particle made of polymer.Such as
Fruit light does not pass through polymer beads, a small amount of polymer can be mixed with the material of such as potassium bromide, needed for which does not absorb
Light in infra-red range, to form disk.
A kind of method for determining polymer content is to re-use representative leather sample, and use can be molten
Solve the solvent extraction polymer of any polymer coating.For example, chlorinated solvent such as methylene chloride or chloroform may dissolve any class
The polymer coating of type, although extracting polymer coating from leather using such solvent with commercial size may be not
Preferably.Solvent can be evaporated to provide solid, thin disk can be formed, or thin disk is mixed and formed with potassium bromide, then permitted
Perhaps the light in infra-red range passes through.This solid can be subjected to FTIR, and obtained spectrum generates the profile of sample, this is a kind of only
Special molecular fingerprint, can be used for easily screening and scanning the sample of many different components.Polymer and plastics FTIR are that one kind has
The analysis instrument of effect, for detecting functional group and characterization covalent bonding information.
Another method that can be used is reflection FTIR.Using this technology, it is several that infrared beam only enters sample surfaces
Micron.If surface is contaminated, solvent washing can be carried out to sample surfaces before carrying out reflection FTIR screening.
The sample of single resin particle size can also be scanned by reflecting FTIR.Sample can be light by reflection FTIR
Test, including polymer beads, opaque sample, fiber, powder and liquid.
In another approach, the sample that grinding pad obtains polymer coating can be used, wherein grinding agent is infrared
There is no the grinding agent of significant absorption in spectrum.Example includes diamond or silicon carbide.For example, Perkin Elmer has one kind to be known as
The FTIR technology of ATR can be completed within short a few minutes.
If desired, the spectral scan of reference material can be generated and store it in library of spectra database.Storage
Reference scan will allow the scanning of materials by all futures to be compared with same early scan.
Unknown infrared spectroscopy is matched with known spectra can manually complete or complete by computer program.Computerization
Spectrum search can in a short period of time quickly more unknown spectrum be located at multiple databases in a large amount of spectrum.
It can provide and be matched with the computerization spectrum of the spectral scan of unknown polymer coating, for example, from most preferably to most
Difference has specified certainty grade.Computer program is for unknown spectral scan to be compared with the scanning of known materials
It is highly useful, but for skilled analytical chemist, check the Spectral matching of computer selection to ensure specimen discerning
Not only accurate but also be completely still helpful.
Although computer matcher can be potentially encountered the difficulty of nuance, all to be used for it is important that determining one group
The chemicals of given polymer coating is removed, and removes a series of polymerizations that condition is usually widely used in every quasi polymer
Object, nuance are unlikely to cause great concern.
Perkin Elmer COMPARE method is to store the representative example of the FTIR database of spectrum, wherein can make
The full light of euclidean is executed with having the search library for multiple storage spectrum of polymer type common in leather processing
Spectrum compares.If desired, the type of polymer can be verified, for example, using SIMCA (the soft independent model of classification classification).This
It is a kind of chemometrics method, it uses comprehensive statistical information.
Using algorithm comparison FTIR spectrum appropriate, such as Perkin Elmer COMPARE algorithm, one can be developed
Spectral evolution library, including intuitive search parameter, with filter to improve the difference between similar material.Like this
System can be used for material identification, emphasize chemical differences using filter appropriate.
The FTIR spectrum library to be compared with the FTIR spectrum of given sample may include 1 to 100,000 spectrum, preferably
1 to 10,000 spectrum, most preferably 1 to 1,000 spectrum.It is relatively fewer in view of the polymer for coating leather, and can
To use same or similar condition to extract the polymer of many types in same category, therefore library does not need very greatly.This
Outside, crucial critical peak, such as the carbamate peak in polyurethane, the ester peak in polyester etc. can be limited to by comparing.
FTIR (Fourier transform infrared spectroscopy) is usually used together with other molecular spectroscopy techniques, including TGA,
DRIFTS, FTIR/TGA, NMR, GC/MS, LC/MS, UV/Vis spectrum, NIR and Raman scattering.It is mentioned in conjunction with the FTIR of these technologies
The important supplement data of the molecular structure about polymer molecule are supplied.When FTIR is used together with these other analytical technologies,
It can effectively identify unknown plastics and polymer material.
Using the common sense of teaching herein and those skilled in the art, the spectrum from unknown polymer coating can analyze
Scanning determines polymer with spectral scan with the scanning for the known materials being stored in computer based library by comparing
Property.Representative relatively (information that Perkin Elmer is provided) of the overlapping FTIR spectrum of PVC polymer is shown in Fig. 1 and 2
In.Library of one of the FTIR spectrum from storage, the other is the sample of screening.
ASTM leather standard
The leather standard of ASTM aids in determining whether, tests and assesses the various physics and chemical property of different form leather.
These standards help the user of leather and fur products all over the world and manufacturer to assess the quality and technique of its material, are made with meeting
With.
The leather standard schedule of ASTM exploitation:
The standard test method (spray test) of D1913-00 (2015) garment-type leather moisture-proof
The standard test method of color fastness and color transfer in the washing of D2096-11 leather
The standard test method of D6014-00 (2015) leather surface dynamic water adsorption measurement
Chemical analysis
The standard test method of total ash in D2617-12 leather
The standard method of test (perchloric acid oxidation) of chromium oxide in D2807-93 (2015) leather
The standard test method of D2810-13 leather pH value
The code test side of D2868-10 (2015) leather, wet blue and wet white nitrogen content (kelvin) and hiding content of material
Method
The standard test method of D3495-10 (2015) leather hexane extraction
D3790-79 (2012) measures the standard test method of leather volatile materials (moisture) with oven method
The standard code of practice that D3897-91 (2012) Chrome Tanning Liquor basicity calculates
The standard test method of chromium oxide in D3898-93 (2015) alkalinity Chrome Tanning Liquor
The standard test method of acidity in D3913-03 (2015) alkalinity Chrome Tanning Liquor
The standard test method of total chloride in D4653-87 (2015) leather
The standard test method of sulfuric acid saline and alkaline in D4654-87 (2015) leather
The standard method of test (total amount, neutrality and Compound-acid) of sulfate in D4655-95 (2012) leather
The standard test method of total solid and content of ashes in D4906-95 (2012) coating material for leather
The standard test method of nitrocellulose in D4907-10 (2015) leather finish
The standard test method of D5356-10 (2015) chrome tanning solution ph
The standard test method of the nitrogen, water that can be extracted in D6016-06 (2012) measurement leather
D6017-97 (2015) measures the standard test method of magnesium sulfate (Epsom salts) in leather
D6018-96 (2012) measures the standard test method of lead salt content in leather
D6019-15 measures the test method (ammonium persulfate oxidation) of chromium peroxide in alkaline Chrome Tanning Liquor
Fat and grease
D5346-93 (2009) measures fat liquor and softens the standard test method of the pour point of petroleum used in compound
The standard test method of the content of ashes of D5347-95 (2012) measurement fat and oil
The standard test method of D5348-95 (2012) sulfonation of dimethylbenzene determination of distillation and sulfated oil water content
D5349-95 (2012) measures the code test of the moisture and volatile content of sulfonation and sulfated oil with hot plate method
Method
The standard test method for the sulfuric anhydride that D5350-95 (2012) is organically combined by titration determination, test method A
D5351-93 (2009) measures the standard test method for organically combining sulfuric anhydride, test method by extraction titration method
B
D5352-95 (2012) organically combines the standard test method of sulfuric anhydride Ash weight measurement, test method C
D5353-95 (2012) measures the standard test method of total desulfurization fatty material
D5354-95 (2012) measures the standard test method of Active principals in sulfonation and sulfated oil
The standard test method of D5355-95 (2012) oil and liquid aliphatic specific gravity
D5439-95 (2012) is used to measure the standard test method of deposit in Moellon
The standard test method of the fusing point of D5440-93 (2009) measurement fat and oil
The standard test method of D5551-95 (2012) measurement valenta value
D5553-95 (2012) measures the standard test method of unsaponifiable matter nonvolatile matter in sulfated oil
The standard test method of the iodine number of D5554-15 measurement fat and oil
In animal used in the fatty wine of D5555-95 (2011) measurement and filling compound, ocean and plant fat and oil
The standard test method of free fatty acid
The moisture contained in fatty and oil in D5556-95 (2011) measurement fat and softening compound and other volatility
The standard test method of substance
The mark of fat and the measurement of contained insoluble impurities in oil in D5557-95 (2011) fat liquor and filling compound
Quasi- test method
The standard test method of the saponification number of D5558-95 (2011) measurement fat and oil
Measurement acidity is free when ammonium or triethanolamine soap is not present in D5559-95 (2011) in sulfonation and sulfated oil
The standard test method of fatty acid/acid value
The standard test method of contained neutral fat substance in D5560-95 (2011) measurement fat and oil
D5562-95 (2011) measures acidity in the presence of ammonium or triethanolamine soap as the examination of free fatty acid/acid value standard
Proved recipe method
D5564-95 (2011) measures the standard test method of total ammonia in sulfonation or sulfated oil
The standard test method of fatty acid condensate solid point in D5565-95 (2011) measurement animal, ocean and plant fat and oil
D5566-95 (2011) measures the standard test method of inorganic salt content in sulphation and sulfonated oil
Vegetables leather
The standard test method of the insoluble ash of D2875-00 (2010) vegetable leather
The standard test method of D2876-00 (2010) vegetable tanned leather water-soluble substances
D4899-99 (2009) vegetable tanning material analytical standard specification
The standard method of test of lignosulfonates (sulfite cellulose) in D4900-99 (2009) tanning extract
D4901-99 (2009) liquid plant tanning extract solution prepares standard schedule
The evaporation of D4902-99 (2009) analytical solution and dry standard test method
The standard test method of total solid and water in D4903-99 (2009) vegetable tanning material extract
D4904-99 (2009) prepares the standard schedule of liquid vegatable tannin extract solution
D4905-99 (2009) prepares the standard code of practice of solid, paste and powdered plant tanning extract solution
D6401-99 (2009) measures the standard test method of non-tannis and tannin in extract in vegetable tanning material
D6402-99 (2014) measures the code test side of soluble solid and insoluble matter in extract in vegetable tanning material
Method
D6403-99 (2014) measures the standard test method of moisture in raw material and waste material
The standard code of practice of vegetable material sampling of the D6404-99 (2014) containing tannin
D6405-99 (2014) extracts the standard code of practice of tannin from raw material and waste material
The standard test method of glycan analysis in D6406-99 (2014) vegetable tanning material
The standard test method of iron and copper analysis in D6407-99 (2014) vegetable tanning material
The standard test method of D6408-99 (2014) process hides liquid analysis
The standard test method of D6410-99 (2014) measurement vegetable tanning liquid acidity
Wet indigo plant
The standard test method of the wet blue stain fungi growth resistance of D4576-08 (2013)
The standard test method of chromium oxide (perchloric acid oxidation) in the wet basket of D6656-14b measurement
The standard test method of the wet blue pH value of D6657-14ael
Standard code of practice of the D6659-10 (2015) for sampling and the preparation of the wet indigo plant of physics and test chemical
The standard method of test of chromium oxide in D6714-01 (2015) ash dampness elimination blue (perchloric acid oxidation)
The fresh or salt that D6715-13 is used to chemically and physically test saves the sampling and preparation of (solidification) rawhide and leather
Standard code of practice
The standard test method of the wet blue or wet white total ash of D6716-08 (2013)
D7476-08 (2013) solidifies the standard test method of (salt preservation) rawhide and skin salt water saturation value
The standard test method of the area stability for the wet indigo plant that D7477-08 (2013) measurement is immersed in boiling water
The standard test method for the resistance that the wet blue surface of D7584-10 (2015) assessment grows fungi in environmental chamber
The standard test method of the wet blue and wet white hexane/petroleum ether extract of D7674-14a
D7816-12 counts the code test side of thermophilic salt and proteolysis bacterium in runway salt water, salt water rawhide and skin
Method
D7817-12 calculates the standard test method of yeast and mould in runway salt water, salt water rawhide and skin
The standard test method of proteolysis count of bacteria in fresh (uncured) rawhide of D7818-12 and skin
The standard test method of yeast and mold count on fresh (uncured) rawhide of D7819-12 and fur
II. chemistry and/or enzymatic treatment removal polymer and other processing
Leather waste is by starting recuperation into suitable treatment reactor.In one embodiment, reactor
It is the column barrel or a series of such buckets of rotation.It is desirable that there is each bucket the material of 50 to 2000 pounds of leather wastes to add
Work ability.
" negative pressure " method can be used to convey material in the system.In this order, gravity is used, because waste material is from each list
First disposed thereon.Then each bucket can be for example closed using pressure seal, and fills chemicals appropriate or a series of
Chemicals, for removing given polymer coating from scrap leather.
Handling chemicals may include for example one or more organic solvents and/or one or more enzymes.Also steaming can be used
Vapour.Chemical penetration leather substance.
Type for the organic chemicals and/or enzyme that remove surface smoothness includes but is not limited to diluted acid or dense neutral salt
Solution.Representative organic solvent includes halohydrin, preferred fluorinated alcohol, such as tetrafluoroethene (TFE) and hexafluoroisopropanol
(HFIP), Hexafluoro acetone, chloropharin, its can with inorganic acid and the aqueous solution of dimethyl acetamide conjugation, preferably comprise lithium chloride,
Ethyl acetate, 2- butanone (methyl ethyl ketone), ether, ethyl alcohol, hexamethylene, water, methylene chloride (methylene chloride), tetrahydrofuran,
Dimethyl sulfoxide (DMSO), acetonitrile, methyl formate and various solvent mixtures.HFIP and methylene chloride are especially desirable molten
Agent.In some embodiments, it adds water in solvent.
In addition, it is generally desirable to solvents to have relatively high vapour pressure to promote electrostatic spinning to penetrate although being not required
The later period of stream stabilizes to generate fiber when solvent evaporates.Once synthetic polymer is removed from leather substance, in these
Each all has " end-of-life " of its own, this is described in subsequent technology relevant to the patent.
It can be used for removing polymer coating from leather waste, not only leather waste can be made to connect with solvent appropriate
Touching, but also leather waste and solvent can be mixed.Mixing may include the stirring with similar type used in washing machine, or
Person may include stirring, alternatively, in preferred embodiments, bucket can slowly rotate.Rotation amount can be based on time, rotation
Number or other suitable methods for determining appropriate endpoint.For example, the types of coatings that can will remove of RLDS data with to use
Enzyme or chemicals type it is associated, and/or removal submit the leather surface processing for recovery needed for rotation number.
Once realizing the removal of leather surface processing, each unit can be rinsed with aqueous fluid, this causes organic poly-
It closes object coating and any organic solvent for removing them is increased on the top surface of aqueous fluid.It then can be such as
By aspirating, being decanted, by from suitably place port discharge or other modes known in the art remove organic coating and/
Or solvent.
Water can be discharged from bucket.If desired, " clean " leather and it is liquid, aqueous can by equipped with centrifugation bag
Centrifuge, the centrifugation bag allow water pass through and retain leather.
Resulting " cleaning " leather substance can be placed on a moving belt now, such as stainless steel grating conveyer,
It can transport next station during leather regeneration there.Alternatively, the movement of other device physicals can be used in it,
Such as cart, fork truck, elevator etc..
For example, once material passes through cleaning region, conveyer can move them into one or more mixing arrangements,
They can connect with the original leather substance of " harmony mix " there, these materials completed from unused synthetic polymer or in advance from
Reason, but it is the waste material in tannery or natural tanning.
Then material tight can be mixed, is then delivered to initial cut device so that leather section pro-fibrotic.
Since their initial stages in the process have unique origin, the uniform mixed of all leather substances is created
It may be especially important for closing object.For example, when " conveying condenser " or hopper with raw material its own is located in it is big mixed
When in mould assembling, it may be implemented closely to mix.The representative size of mixing cassette is about 10 feet wide, 20 feet long, but according to required
Greater or lesser box can be used in output.
Incorporating a material into mixing tank can be realized by negative pressure, such as gravity.In the one aspect of the embodiment, make
Keep material mobile by pipeline work with air pressure, wherein to allow material to fall into mixed in the variation of the air pressure of desired locations
In mould assembling.
In one embodiment, the skirtboard of spine is used to fetch material from one end of box, and is pneumatically conveyed
Into vertical transmission unit.This can cause the cross section of material to become harmonious mixture, and preparation is delivered to next pre- fibre
The process of dimensionization.Operation permission is uniformly mixed in the remainder of the process.
The processed leather waste of fibrosis
The leather waste of purifying is optionally closely mixed with original leather, then moves to a station, it can there
With fibrosis, and according to its final finished application humidification and/or moisten.
In processed Leather Waste fibrosis and before being transformed into yarn, prepare Leather Waste to receive humidity and lubrication
It is very important.In one embodiment, moisturizer or surfactant are used in a region, in the second area
Use lubricant.In another embodiment, moisturizer and surfactant are used to single area.It may be preferred, however, that
Using individual region, because if handling leather in separated region, then more easily recycling/recycling across leather
Moisturizer/surfactant.
In one embodiment, prime area or surfactant region occur before fibrosis, and lubricate in fibre
Occur after dimensionization.
Temperature control is all critically important in the two regions.These processing regions are the committed steps during this, will be skin
Leather fiber and webbing carry out flexibility." surfactant area " uses rotary blender, is formed on leather and fur products uniform
Mixture is handled, and moisturizer is added in leather by steam and lubricant.
It is recommended that the vapor (steam) temperature in surfactant region is no more than 135 DEG C.The egg of the Optimal pH with 9-10 can be used
The various selections of white enzyme and/or surfactant promote the moisture absorption of skin/hide/fiber.Representative protease include but
It is not limited to fungal proteinase, pepsin, trypsase, chymotrypsin, papain, bromelain and withered grass bar
Mycoproteinase.
In the case where processed waste material is the finishing of process for tanning, it is poly- to remove synthesis not need initial cleanness fiber
Object is closed, so if needing closely to be mixed, raw material can flow directly to close mix stages, and can be living by surface
The further processing of the area Xing Ji.
Once completing the process, material being removed from catalytic steam unit and transporting to can reduce leather chip
The region of size.
Material is moved to " cutting area " from " surfactant area " although any transportation resources appropriate can be used,
In one embodiment, using conveyer.
In one embodiment, waste material reduces size in two individual stages.In the first phase, waste material is cut
At size of the length and width between about 0.5 and about 3 inch, and generally square or rectangle.
The scantling of initial stage reduces all subsequent fibres that can be carried out by cutting machine, and be generated by the effect
Dimension (length is less than 3mm) can filter out during this.Then length can be moved into secondary add less than the segregation fiber of 3mm
They are used to be suitble to the final use of its size by work in this process.
By making material by the closing tunnel equipped with series or rotating knife, secondary stock reduction can occur.Another
In one embodiment, material can pass through the cylinder pair with wire or small pin.Pairs of cylindrical body is to comb or extract
The mode of fiber rotates inward.In the third embodiment, material can be under the cylindrical cuts head with spiral cutting sword
Side passes through.The edge of cutting device has the sharp projection along spiral ridge, also functions to the combing and extracting method of fiber
Effect.If desired, may then pass through rotary cutting blade further refines gained fiber, to allow more accurate fiber
Length processing.
It is by fiber back to process of the length between 3mm to 9mm that the fiber, which reduces the emphasis at station, this depends on downstream
Application requirement.It should be less than less than 5% total fiber 3 millimeters long, the fiber less than 3% should be longer than 9 millimeters, and good fiber quality length is
Needed for high quality non-woven fabrics leather replaces product, having a size of 6 millimeters to 7 millimeters.For example, if final fiber applications are skins
Yarn spinning is removed from office, then best fibre length will be between 4mm and 6mm.
Once leather waste is reduced in size to fiber, and fiber size is suitable, and fiber can wetted and/or profit
It is sliding.Lubrication generates drapability, flexibility and intensity.Leather in native state is non-woven material, wherein the fibril of fiber
Dimension is grown together.After fibrosis, natural leather is deconstructed.It is natural non-by returning to fiber in the regeneration of the product
Weaving material is advantageous to rebuild natural appearance.Leather manufacture be using acid, alkali, salt, enzyme and tannin come dissolved fat and
Nonfibrous protein and the science for reinforcing the combination between collagenous fibres.The purpose can be for example, by right in the first treatment region
Leather fiber carries out rehydrated realize.Salt can be used for cleaning fiber, and enzyme and tannin can be replaced, so as to from eventually for filling out
Restore more crude in the substance for burying or burning.
In one embodiment, contact leather fiber with protease or other enzymes using treatment region, this is conducive to skin
It removes from office fiber and absorbs tannin and/or lubricating oil.
The etymology of " tannin " this word is very ancient, reflects a kind of rich in traditional technology." tanned " (waterproof and preservation)
It is that animal's leather is converted leather by plant extracts and its various parts for describing by using different plant species
The word of process.A series of tannin can be used during processing, the vegatable tannins such as including Pyrogallol, it is by two types
Polyphenol system composition: Hydrolysable Tannins (pyrogallol class), main component be glucose and acid, as chelate, tan flower,
Gallic and m-digallic, and the condensation based on leucocyanidin and the similar substance to be linked together in a manner of not knowing
(catechol) tannin.Pyrogallol tannin can by acid or enzyme hydrolysis, including gall tannin (come from plant goitre) and Ellagitannins,
It is characterized in that divi divi, myrabolans, sumac, tara, valonea and other well-known tannin.Condensed tannin
Non-hydrolysable, and be the feature of Chinese hemlock spruce, mangrove, white birch, wattle etc..Condensed tannin is more puckery, i.e. their neighbour benzenetriols
It quickly shines into, there is bigger molecule, and resiliency is poor.These can add or not add one or more enzymes
It is put into leather in aqueous solution.
Floristic example for obtaining tannin in tannery is Wattle (Acacia sp.), oak (oak category
Plant), eucalyptus (Eucalyptus sp.), birch (Betula sp.), willow (Salix Caprea), pine tree (Pinus
) and Quebracho (Scinopsis Balansae) sp..The most important aspect for selecting tannin is that high molecular weight and high conformation are moved
Shifting rate.
Oil is added usually after adding tannin.Oily re-lubrication leather fiber.The example for the oil that can be used includes but not
It is limited to neatsfeet oil, ermine oil and product such as Meropol Oil 805.
In one embodiment, fiber is mixed with oil, and penetrates into oil in fiber.It is preferred real at another
It applies in scheme, fiber is contacted with steam, and steam can be high steam, and fiber is allowed to be swollen.The water content of fiber is ideally
Rise to the about 10-30% of fibre weight.Then, once fiber is swollen, just oil is applied on fiber, and fiber can be compared
Preferably permeable fiber before swelling.Fiber is swollen with steam first, then with one or more chemicals/enzyme dipping method
Referred to herein as " catalytic steam " method.Although water is not real catalyst, it is not real reactant, but its meeting
Make filament expansion, it facilitates the infiltration of chemical substance/enzyme, then when fiber is restored to the ambient water of about 6% to about 8% moisture
It is removed when point content.
These oil ideally no more than 125 DEG C at a temperature of be added in leather fiber.It is recommended that the residence time be about 2 to
12 hours.After the residence time appropriate, material can be sent to final packaging and be transferred to secondary processing process, there will
Fiber is converted into finished product.
Content according to the above disclosure, those skilled in the art can carry out modification and change appropriate to the embodiment above
Change.Therefore, the present invention is not limited to above disclosures and the embodiment.Modifications of the present invention and change should be fallen by weighing
Benefit requires in the scope of the present invention limited.In addition, although having used certain technical terms, technology throughout the specification
Term is intended to be easy to explain, rather than limit the invention in any way.
Claims (10)
1. it is a kind of by after industry or consumption after waste leather material manufacture leather fiber method, comprising:
A) obtain have surface smoothness industry after or consumption after waste leather material amount,
B) the waste leather material is handled to remove all or almost all surface smoothnesses,
C) the waste leather material is cut into the size of about 0.5 to about 3 inchage and width,
D) surfactant is added in the waste leather material of cutting,
E) cut the waste leather material of the cutting so that the dimensions length of at least about 92% total fiber 3mm to 9mm it
Between, it is less than the 5% of 3mm less than total fiber length, and be more than the 3% of 9mm less than total fiber length, to form leather fibre
Dimension, and
F) moisturizer and/or lubricant are added in the leather fiber.
2. method described in claim 1, wherein before moisturizer and/or lubricant is added, using steam to the fiber
It is handled.
3. method described in claim 1, wherein polymer coating is selected from.
4. method described in claim 1, wherein the solvent for removing surface covering is selected from representative organic solvent, packet
Include: halohydrin, preferred fluorinated alcohol, such as tetrafluoroethene (TFE) and hexafluoroisopropanol (HFIP), Hexafluoro acetone, chloropharin, they can be used
It is used in combination in the aqueous solution of inorganic acid and dimethyl acetamide, preferably comprises lithium chloride, ethyl acetate；2- butanone (methyl
Ethyl ketone), ether；Ethyl alcohol；Hexamethylene；Water；Methylene chloride (methylene chloride)；Tetrahydrofuran；Dimethyl sulfoxide (DMSO)；Second
Nitrile；Methyl formate and various solvent mixtures.HFIP and methylene chloride are especially desirable solvents.In some embodiments,
It adds water in solvent.
5. method described in claim 1, wherein surfactant is anion, nonionic, cation or amphoteric ion surface
Activating agent.
6. method described in claim 1, wherein moisturizer and/or lubricant are neat's foot oil, ermine oil or Meropol Oil
805。
7. method described in claim 1, wherein surface covering is polyurethane or polyvinyl chloride.
8. method described in claim 1 further comprises carrying out reflection FTIR analysis to the waste leather material, to determine
Remove the types of coatings before coating.
9. method according to any one of claims 8, wherein there are more batches of waste leather materials, and by batch with same or similar coating
Material combination uses the solvent system for being specifically used for dissolving specific coating to remove coating for handling.
It further comprise that will remove the waste leather material and original leather substance of coating 10. method described in claim 1
Close mixing, forms the random mixture of processed waste leather material and original leather substance.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US201662305260P | 2016-03-08 | 2016-03-08 | |
| US62/305,260 | 2016-03-08 | ||
| PCT/US2017/020141 WO2017155756A1 (en) | 2016-03-08 | 2017-03-01 | Process for preparing fibers for use in rejuvenated leather substrates |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109477255A true CN109477255A (en) | 2019-03-15 |
Family
ID=59789767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201780028381.6A Pending CN109477255A (en) | 2016-03-08 | 2017-03-01 | Method of the preparation for the fiber of regenerative leather substrate |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US20190078233A1 (en) |
| EP (1) | EP3426831A4 (en) |
| CN (1) | CN109477255A (en) |
| IL (1) | IL261689A (en) |
| RU (1) | RU2018135024A (en) |
| WO (1) | WO2017155756A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021145599A1 (en) * | 2020-01-13 | 2021-07-22 | 주식회사 아코플레닝 | Leather fiber for leather-spun yarn |
| EP4163401A4 (en) * | 2021-08-26 | 2023-11-22 | Atko Planning Inc. | Leather fiber for leather spun yarn having improved physical properties |
| EP4379066A1 (en) * | 2022-10-12 | 2024-06-05 | Atkoplanning Inc. | Product material leather fabrics physically extracted from cowhide |
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- 2017-03-01 CN CN201780028381.6A patent/CN109477255A/en active Pending
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Also Published As
| Publication number | Publication date |
|---|---|
| EP3426831A4 (en) | 2020-05-06 |
| EP3426831A1 (en) | 2019-01-16 |
| WO2017155756A1 (en) | 2017-09-14 |
| IL261689A (en) | 2018-10-31 |
| RU2018135024A (en) | 2020-04-08 |
| US20190078233A1 (en) | 2019-03-14 |
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